CN1167257A - Method for indicating metallographic texture of gap-free atom cold rolled annealed steel - Google Patents

Method for indicating metallographic texture of gap-free atom cold rolled annealed steel Download PDF

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Publication number
CN1167257A
CN1167257A CN 97100731 CN97100731A CN1167257A CN 1167257 A CN1167257 A CN 1167257A CN 97100731 CN97100731 CN 97100731 CN 97100731 A CN97100731 A CN 97100731A CN 1167257 A CN1167257 A CN 1167257A
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reagent
rolled annealed
polishing
steel
cold rolled
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CN 97100731
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李安华
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Baoshan Iron and Steel Co Ltd
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Baoshan Iron and Steel Co Ltd
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Priority to CN 97100731 priority Critical patent/CN1167257A/en
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Abstract

The present invention discloses a display method for cold-rolled annealed gapless atomic steel metallurgical structure, including: making ground sample pass through such processes of polishing and etching treatment at the same time to remove interference layer; then pre-eatching with alcohol nitrate as reagent No.1, and using reagent No.2 composed of 1-10% sodium metabisulfite, 3-20% anhydrous sodium thiosulfate and distilled water (the rest) to make eatching until the test surface is completely changed into light blue color; then rinsing and wiping the light blue surface, drying, then can make metallurgical observation and take pictures. For cold-rolled annealed IF steel metallurgical sample prepared by said invented method, its fertitic crystal position can be clearly and comprehensively displayed. Besides, it has no color, dimorphic boundary or false image.

Description

Method for displaying metallographic structure of cold rolled annealed gapless atomic steel
The present invention relates to a kind of polishing etch method for preparing metallographic sample.
Gapless atomic steel (IF steel) is the novel punching press steel of a kind of Ultra-low carbon, super deep-draw, is extensively utilized with its good mouldability, hot dip galvanizing process performance industries such as auto industry, light industry and household electrical appliance at home and abroad.The main content of examination of IF steel microscopic examination is a grain size, because of its steel quite pure, and after cold rolled annealed its crystal grain form special position to, adopt on the test face of conventional microscopic examination method and conventional reagent preparation, having greatly, crystal boundary can not show, for the Ti-IF steel, the Ti-Nb-IF steel, its Display of Grain Boundary is just difficult more, because Display of Grain Boundary is not entirely for the grain size size of IF steel, other examination of level brings very big difficulty, and the crystal boundary of the cold rolled annealed IF steel of comprehensive clear demonstration to be IF steel further investigation press for the problem of solution, and do not see the report that this difficult problem is resolved in the domestic and foreign literature so far.
The objective of the invention is to obtain a kind of cold rolled annealed IF steel method for displaying metallographic structure, can be with comprehensive clear the showing of ferrite crystal boundary, to solve the problem of IF steel examination nucleus degree size.
The object of the present invention is achieved like this:
A kind of method for displaying metallographic structure of cold rolled annealed gapless atomic steel is after metallographic sample is used the sand paper grind away,
(1) polishing: when polishing with antiscuffing paste, corroded 0.5~5 second in composition (weight) is the reagent 1 of 1~5% nitric acid alcohol, polish after then rinsing with clean flowing water again, the edge polishing marginal rot loses 3~6 times repeatedly like this, then,
(2) pre-etching: pre-etching is 10~30 seconds in reagent 1, then,
(3) corrosion: at composition (weight) be: 1~10% Sodium Metabisulfite, 3~20% Sodium Thio Sulphate(Anhydrous)s, all the other are for corroding in the reagent 2 of distilled water when test face all is sky-blue, sample taken out from reagent 2 limit washes down, the limit is wiped examination gently and can be observed after sky-blue is all removed, drying up.
Sodium Metabisulfite in the reagent 2 can replace with potassium metabisulfite.
In edge polishing marginal rot etching method, gently corrode 0.5-5 second with 1-5% nitric acid alcohol.
Etching time in reagent 2 is 30~100 seconds.
Below in conjunction with accompanying drawing the present invention is further described.
The grain structure that Fig. 1 adopts the conventional method corrosion to show.
The grain structure of Fig. 2 for using the inventive method corrosion to show.The composition of sample is Ti, the Nb-IF steel, and its composition (percentage by weight) is: C:0.0054, Si:0.03, Mn:0.15, P:0.008, S:00062, Nb:0.014, N:0.0029, Ti:0.051, enlargement factor is 200 times.
Cold rolled annealed IF steel is because its special texture is often used conventional nitric acid alcohol reagent Display of Grain Boundary is complete (such as Fig. 1) not, and the present invention uses reagent 1 to carry out pre-etching, uses then reagent 2 Corrode, any color and vacation do not appear in the ferritic structure that obtains cold rolled annealed IF steel Resemble, make crystal boundary obtain comprehensive clear demonstration.
Method of the present invention is at first sample to be carried out polishing behind the grind away, because low-carbon and low-alloy Steel is after cold rolled annealed, and its metallographic specimen often easily produces the shallow shape that is charred of one deck when polishing Interfere with layer, this interfere with layer is not removed, and the test face after corrosion is just very unintelligible, and the IF steel is Ultra-low carbon, extra-deep drawing steel, this problem is more outstanding. For removing this interfere with layer, the present invention Adopt the step of edge polishing marginal rot erosion, namely carefully polish with diamond paste earlier, exist then 1~5% nitric acid, all the other corroded 0.5~5 second in the reagent 1 of absolute ethyl alcohol, used rapidly then Flowing water is rinsed well, polish again, like this edge polishing marginal rot erosion, repeatedly 3~6 times until Remove interfere with layer fully. The concrete technology parameter can be slapped flexibly according to the weight of operator's hand strength Hold, if the operational degree of edge polishing marginal rot erosion too gently can not be removed interfere with layer, degree fully Excessive, original one deck interfere with layer is removed and is produced new interfere with layer.
Etch process among the present invention was divided into for two steps carries out, and at first carries out pre-etching, adopts examination Agent 1 is 1~5% nitric acid alcohol, and this reagent is a kind of corrosion reagent of routine, the time is 10~30 seconds, the pre-etching degree was according to different components and different conditions (annealing temperature, the insulation of sample Time, the type of cooling etc.) take the circumstances into consideration to grasp, corrode too shallowly, also have not in the corrosion below Few Display of Grain Boundary does not go out, and is too dark, twin boundary can occur on the test face, all twin boundaries that occurs Test face, its sample must get again preparation, and must must return at least 800# water In the grind away stage of sand, could eliminate twin boundary fully. Rapid with the sample after reagent 1 pre-etching Flushing dries up to be placed on and continues corrosion in the reagent 2, and the composition of reagent 2 (percentage by weight) is: 1~10% Sodium Metabisulfite or potassium metabisulfite, 3~20% Sodium Thio Sulphate(Anhydrous)s, All the other are distilled water, and corrosion is until test face all is sky-blue, and the time is generally 30~100 Second, rapidly sample is taken out then the limit and use flowing water irrigation tests face limit with clean from reagent 2 Absorbent cotton dabs test face, blows immediately after one deck sky-blue on the test face is cleaned rapidly Do, the metallographic specimen for preparing can be placed on metallography microscope Microscopic observation or photograph.
The present invention uses reagent 2 and reagent 1 combination, can make the ferrite group of cold rolled annealed IF steel Knit any color does not appear and only these special bit to form one deck thin in the grain boundary Film, when the white light of continuous spectrum composition projects on the grain boundary with this film, its In have good position phase condition and the amplitude condition with destructive interference of light positive of a wavelength to meet, then this Plant wavelength and just eliminate fully, the reverberation on the grain boundary of IF steel is white no longer just at this moment Light, and the therewith corresponding complementary color of wavelength (also claiming interference colours) has appearred, thus make cold rolled annealed The grain boundary of IF steel obtains comprehensive clear demonstration.
Introduce embodiments of the invention below.
After will throwing with 2.5 μ diamond pastes are smart with the sample that sand paper grinds, in 2% nitric acid alcohol reagent, corroded 1~2 second, polishing again after washing down with flowing water, edge polishing marginal rot erosion is repeatedly after 3 times like this, pre-etching is after 20 seconds in 2% nitric acid alcohol reagent, with sample rapidly flushing dry up and be placed on composition (weight) and be: 2% Sodium Metabisulfite, 6% Sodium Thio Sulphate(Anhydrous), all the other are corrosion 50 seconds in the reagent 2 of distilled water, when test face all is sky-blue, sample is taken out the limit dab test face with clean wet absorbent cotton from reagent 2 with flowing water irrigation tests face limit, dry up immediately after one deck sky-blue on the test face cleaned rapidly, on metaloscope, observe, photograph obtains photo such as Fig. 2 shows.
Compared with prior art, the cold rolled annealed IF steel metallographic sample for preparing with the inventive method Ferrite crystal grain obtains comprehensive clear demonstration, does not have twin boundary, color and illusion, at the bottom of the photo Son is very clean.

Claims (4)

1. a method for displaying metallographic structure of cold rolled annealed gapless atomic steel at first is with behind the metallographic sample usefulness sand paper grind away, it is characterized in that:
(1) polishing: when polishing with antiscuffing paste, etch is 0.5~5 second in reagent 1: 1~5% nitric acid alcohol, polishes again after then rinsing with clean flowing water, and edge polishing like this, marginal rot erosion 3~6 times repeatedly, then,
(2) pre-etching: pre-etch is 10~30 seconds in reagent 1, then,
(3) corrosion: at composition is 1~10% Sodium Metabisulfite, 3~20% Sodium Thio Sulphate(Anhydrous)s, all the other are for corroding in the reagent 2 of distilled water when test face all is sky-blue, sample taken out from reagent 2 limit washes down, the limit is wiped examination gently and can be observed after sky-blue is all removed, drying up.
2. method for displaying metallographic structure according to claim 1 is characterized in that: the Sodium Metabisulfite in the described reagent 2 can replace with potassium metabisulfite.
3. method for displaying metallographic structure according to claim 1 is characterized in that: in the described edge polishing marginal rot etching method, light corrosion is 0.5~5 second in 1~5% nitric acid alcohol.
4. method for displaying metallographic structure according to claim 1 is characterized in that: the etching time in reagent 2 is 30~100 seconds.
CN 97100731 1997-02-27 1997-02-27 Method for indicating metallographic texture of gap-free atom cold rolled annealed steel Pending CN1167257A (en)

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CN 97100731 CN1167257A (en) 1997-02-27 1997-02-27 Method for indicating metallographic texture of gap-free atom cold rolled annealed steel

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101936838A (en) * 2010-09-17 2011-01-05 马鞍山钢铁股份有限公司 Bainite steel color metallurgical-phase dye and color display method thereof
CN101984334A (en) * 2010-10-29 2011-03-09 河北钢铁股份有限公司唐山分公司 Method for displaying metallurgical structure of ultralow-carbon cold roll annealed interstitial-free steel
CN102374991A (en) * 2011-09-22 2012-03-14 首钢总公司 Quantitative analyzing method for cementite in automobile plate
CN102890027A (en) * 2012-09-29 2013-01-23 攀钢集团攀枝花钢铁研究院有限公司 Metallographic structure display method of interstitial free (IF) steel cold-rolled sheet containing titanium (Ti)
CN103308514A (en) * 2013-05-09 2013-09-18 中原特钢股份有限公司 Method for detecting carbide nonuniformity of tool steel by annealed room-temperature etching method
CN108240933A (en) * 2017-12-11 2018-07-03 囯网河北省电力有限公司电力科学研究院 A kind of high-purity aluminium microstructure morphology etchant and corrosion method
CN111458208A (en) * 2020-03-25 2020-07-28 唐山钢铁集团有限责任公司 Display method for distinguishing cold-rolled annealed multiphase steel structure

Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101936838A (en) * 2010-09-17 2011-01-05 马鞍山钢铁股份有限公司 Bainite steel color metallurgical-phase dye and color display method thereof
CN101984334A (en) * 2010-10-29 2011-03-09 河北钢铁股份有限公司唐山分公司 Method for displaying metallurgical structure of ultralow-carbon cold roll annealed interstitial-free steel
CN102374991A (en) * 2011-09-22 2012-03-14 首钢总公司 Quantitative analyzing method for cementite in automobile plate
CN102374991B (en) * 2011-09-22 2013-04-17 首钢总公司 Quantitative analyzing method for cementite in automobile plate
CN102890027A (en) * 2012-09-29 2013-01-23 攀钢集团攀枝花钢铁研究院有限公司 Metallographic structure display method of interstitial free (IF) steel cold-rolled sheet containing titanium (Ti)
CN103308514A (en) * 2013-05-09 2013-09-18 中原特钢股份有限公司 Method for detecting carbide nonuniformity of tool steel by annealed room-temperature etching method
CN103308514B (en) * 2013-05-09 2015-08-19 中原特钢股份有限公司 A kind of method adopting annealed state normal temperature etch testing tool steel carbonide unevenness
CN108240933A (en) * 2017-12-11 2018-07-03 囯网河北省电力有限公司电力科学研究院 A kind of high-purity aluminium microstructure morphology etchant and corrosion method
CN108240933B (en) * 2017-12-11 2021-10-22 囯网河北省电力有限公司电力科学研究院 Ultra-pure aluminum microstructure morphology etching agent and etching method
CN111458208A (en) * 2020-03-25 2020-07-28 唐山钢铁集团有限责任公司 Display method for distinguishing cold-rolled annealed multiphase steel structure

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